Co(en) 3V 3O 6·H 2O has been synthesized by using hydrothermal method and characterized by IR, ICP, XPS and X ray diffraction analysis. The results of the X ray diffraction analysis show that structure of Co(en) 3(VO 3) 3·H 2O is orthorhombic with P2(1)2(1)2(1) , and the crystal data are a =0 819 2(7) nm, b =1.263 9(1) nm, c =1.804 8(2) nm, V =1.868 8(3) nm 3, Z=4, D c=1.973 g/cm 3, F (000)=1 124, R 1=0.040 7, wR 2=0.094 9, ( Δ/ρ ) max =706 e/nm 3 and ( Δ/ρ ) min =-452 e/nm 3. The results of XPS show that the Co 2+ was oxidized to Co 3+ (en) 3 at about pH=7.0 in the aqueous solution.
The title compound [N(CH 3) 4] 4 [H 5PMo 5V 9O 42 ] ·3.5H 2O was synthesized by hydrothermal method and its structure was determined with single crystal X ray analysis. The cluster anion is a bicapped Keggin polyanion, two vanadium atoms are distributed at two capping metal atom positions. The crystal is monoclinic, space group C2/c with a=1.284 8(4) nm, b=2.366 4(4) nm, c=2.113 6(4) nm, β= 90.69(2)° , V=6.425(4) nm 3, Z=4, D c=2.07 g\5cm -3 , R=0.066, R w=0.069, S=1.33, \{(Δ/σ) max =\}0 04, \{(Δρ) max =\}91 e·nm -3 .
